CN104844178B - Add the preparation method of the self-lubrication ceramic cutter material of spherical nano-silicon dioxide cladding hexagonal boron nitride composite granule - Google Patents
Add the preparation method of the self-lubrication ceramic cutter material of spherical nano-silicon dioxide cladding hexagonal boron nitride composite granule Download PDFInfo
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Abstract
The present invention relates to the preparation method of a kind of self-lubrication ceramic cutter material adding spherical nano-silicon dioxide cladding hexagonal boron nitride composite granule.In described self-lubrication ceramic cutter material, each raw material components percent by volume is: TiC 15 75%, h BN@SiO22 20%, MgO 0.2 2.5%, remaining is Al2O3；h‑BN@SiO2It is that h BN powder body is scattered in dehydrated alcohol the preparing spherical SiO 2 cladding lamellar hexagonal boron nitride composite granule prepared in 30 70 DEG C of dropping tetraethyl orthosilicates.The present invention also provides for the preparation method of described self-lubrication ceramic cutter material.Add h BN@SiO2Wettability, minimizing pore and h BN self reunion of h BN and matrix can be improved, its mechanical property is improved while keeping the excellent lubrication property of cutter material, reduce h BN adds the adverse effect to self-lubrication ceramic cutter material mechanical property, in addition to being applicable to make self-lubrication ceramic cutter, may further be used to make ceramic die, bearing and other abrasion-proof corrosion-proof parts.
Description
Technical field
The present invention relates to self-lubrication ceramic cutter material, particularly to the preparation method of a kind of self-lubrication ceramic cutter material adding spherical nano-silicon dioxide cladding hexagonal boron nitride composite granule.
Background technology
Self-lubrication ceramic cutter has good lubrication property, the coefficient of friction between cutter and workpiece material can be substantially reduced, the unification of sintex anti-attrition and wearability is realized in the case of the most additional lubricating fluid, this makes self-lubrication ceramic cutter be particularly suited for being not added with the dry cutting of cutting fluid, has a wide range of applications in modern processing.
Being added to mutually in ceramic cutting tool material matrix as interpolation by kollag is one of effective way realizing cutter self-lubricating function.Hexagonal boron nitride (h-BN) is the kollag of a kind of function admirable, can be used for the kollag in self-lubrication ceramic cutter material.But directly h-BN or other kollags are added to and ceramic matrix also result in while realizing material self-lubricating function being remarkably decreased of material mechanical performance.The TiB prepared such as Xu Xiuguo etc.2/ WC/h-BN self-lubricating ceramic material, after adding h-BN, the frictional behaviour of material has had bigger improvement, but its mechanical property is also decreased obviously, and particularly bending strength have dropped 21%, sees the .TiB such as Xu Xiuguo, Xu Chonghai, Fang Bin2The preparation of/WC/h-BN self-lubricating ceramic material and mechanical property [J]. material engineering, 2014, (4): 63-67.Therefore, it is achieved the unification of self-lubricating solid ceramic cutting tool material intensity and greasy property had become the important topic of self-lubrication ceramic cutter material technological improvement already.
The mechanical property of solid lubricant particle own is relatively low, and be combined the tightst, easy reunion etc. with matrix be to cause self-lubrication ceramic cutter material mechanical properties decrease main cause.Ding Guangyu etc. have studied the interpolation nickel coated graphite impact on Fe based self lubricating composites performance, research shows to add the mechanical property of nickel coated graphite composite material and tribological property is substantially better than the composite adding uncoated graphite, see fourth light beautiful, Jia Cheng factory, Miao Xiaoli etc., the research of new iron-based solid self-lubricating composite material tribological property, [J]. PM technique, 2010,28 (2): 110-114.Wei little Feng etc. are in order to improve the wettability between hexagonal boron nitride (h-BN) kollag and Ni-Cr alloy matrix, use nickel nitrate to decompose hydrogen reduction method and prepare Ni cladding h-BN powder, obtain tissue evenly, the self-lubricating composite that interface cohesion between kollag and matrix is good, see Wei little Feng, Wang Chu, Feng Yan etc. the impact [J] on Ni-Cr/hBN solid self lubricant material performance of hexagonal boron nitride (hBN) plating nickel on surface. Materials Science and Engineering of Powder Metallurgy, 2011,16 (5): 665-670.The composite of above Ni cladding is applicable to ferrous alloy (Fe-Ni-Cu-Mo) self-lubricating composite and Ni-Cr alloy self-lubricating material, is unsuitable for alumina base or TiB2Base self-lubricating ceramic cutting tool material.
Summary of the invention
For the deficiencies in the prior art, the present invention provides the preparation method of a kind of self-lubrication ceramic cutter material adding spherical nano-silicon dioxide cladding hexagonal boron nitride composite granule, and while the method for the present invention can make self-lubricating ceramic material obtain good lubrication characteristic, mechanical property is also improved.
Term illustrates:
In the present invention, spherical nano-silicon dioxide cladding lamellar hexagonal boron nitride, is abbreviated as h-BN SiO2。
The technical solution used in the present invention is as follows:
A kind of spherical nano-silicon dioxide that adds is coated with lamellar hexagonal boron nitride (h-BN SiO2) preparation method of self-lubrication ceramic cutter material of composite granule, in described self-lubrication ceramic cutter material, each raw material components percent by volume is:
TiC 15-75%, h-BN@SiO22-20%, MgO 0.2-2.5%, remaining is Al2O3；
Comprise the following steps that
(1)h-BN@SiO2The preparation of composite granule:
In the dehydrated alcohol that the h-BN powder body that particle diameter is 1-20 μm is scattered in, h-BN is 0.5-10g:100-500mL with the mass volume ratio of dehydrated alcohol, ultrasonic disperse 10-30min, then add suitable quantity of water and to regulate pH value with the ammonia of mass fraction 23-28wt% be 8-9.5, by the mixed liquor magnetic agitation obtained heating in water bath, temperature is maintained at 30-70 DEG C；Being slowly added dropwise tetraethyl orthosilicate (TEOS), h-BN is 0.5-10g:6-50mL with the mass volume ratio of tetraethyl orthosilicate, and tetraethyl orthosilicate rate of addition is 0.02-0.6mL/min, and the response time is 2-24h；The suspension centrifugation 5-40min under the conditions of 1000-4000r/min that will obtain, with washes of absolute alcohol 2-5 time, is vacuum dried under the conditions of 40-100 DEG C, obtains with micron h-BN as core, Nano-meter SiO_22Preparing spherical SiO 2 for shell is coated with lamellar hexagonal boron nitride (h-BN SiO2) composite granule；
(2) Al is weighed in proportion2O3And TiC powder, it is scattered in respectively in dehydrated alcohol, ultrasonic disperse mechanical agitation 10-30min, by gained Al2O3Suspension adds MgO powder, again ultrasonic disperse mechanical agitation 10-30min, the complex phase suspension being uniformly mixed after mixing with TiC suspension；
(3) above-mentioned complex phase suspension being poured into ball milling fill, add sintered carbide ball, ball material mass ratio is 8-12:1, is filled with nitrogen or argon as protective atmosphere continuous ball milling 36-72h；
(4) h-BN@SiO it is proportionally added into2Composite granule ball milling 1-3h again, gained ball milling liquid continuous drying 24-48h at 100-120 DEG C in vacuum drying oven, then sieve and obtain mixed powder, seal standby；
(5) the mixed powder loading graphite jig being dried by step (4) gained carries out hot pressed sintering, sintering temperature 1600-1700 DEG C, hot pressing pressure 25-35MPa, temperature retention time 10-30min, programming rate 10-20 DEG C/min.Obtain the self-lubrication ceramic cutter material of the present invention.
According to currently preferred, raw material components percent by volume is: the volumn concentration of described TiC is 25-50%；Described h-BN@SiO2Volumn concentration be 4-12%；The volumn concentration of described MgO is 0.4-1.2%.
Preferably, described Al2O3, TiC and MgO be micron order；More preferably Al2O3The particle diameter of powder is 0.2-2 μm, and the particle diameter of TiC powder is 0.2-1.5 μm.
According to currently preferred, adding suitable quantity of water described in step (1) is distilled water, and amount of water is 0.5-10g:4-30mL with the mass volume ratio of h-BN.
Preferably, in step (2), the mass volume ratio of h-BN and tetraethyl orthosilicate is 1-5g:12mL-36mL.12mL-36mL tetraethyl orthosilicate is divided into 3 parts, in 1.5h, is slowly added dropwise the tetraethyl orthosilicate of a deal by several times；Continue reaction 0.5h for the first time after dropping, then second time drips the tetraethyl orthosilicate of a deal in the same way；After completing to drip for the second time, continuing reaction 0.5h, third time drips the tetraethyl orthosilicate of a deal the most in the same way；Third time continues reaction 0.5h after being added dropwise to complete, total reaction time is 6h.
According to currently preferred, the sintered carbide ball described in step (3) is YG6 or YG8, and market is commercially available.
The present invention is with aluminium oxide (Al2O3) it is matrix, titanium carbide (TiC) is for strengthening phase, with h-BN@SiO2For kollag, with magnesium oxide (MgO) as sintering aid, through the self-lubrication ceramic cutter material that hot-pressing sintering technique is prepared from.Especially with the cladded type composite granule h-BN@SiO with nucleocapsid structure2For kollag, the physical and chemical performance of covering material and encapsulated material can be taken into account, micron-stage sheet-like h-BN is coated with one layer can combine closely with matrix, wettability is good and the material SiO that should not reunite2, improve the problem of cutter material mechanical properties decrease present in kollag use process, and h-BN SiO2Clad complete, fine and close, be tightly combined, more than ultrasonic disperse 20min is all without destroyed.
The present invention compared with prior art has the advantage that
1, the present invention is by adding h-BN@SiO2As kollag, in working angles, one layer can be formed on sintex surface containing h-BN, SiO2And Fe2O3Friction film, significantly reduce the coefficient of friction of cutter material, improve the friction and wear behavior of material.Due to the laminated structure of h-BN, the growth of material internal crystal grain can be suppressed；The multiple mechanism synergism such as crack deflection, crackle branch, crackle bridging, improve the fracture toughness of material jointly.Additionally, its high temperature oxidation resistance of h-BN is more preferable, can be until still there is good self-lubricating property within the temperature range of 900 DEG C.
2, the present invention adds SiO2Modified h-BN kollag, utilizes hot-pressing sintering technique to be prepared for self-lubrication ceramic cutter material, compared with the self-lubrication ceramic cutter material directly adding h-BN, adds h-BN@SiO2Can improve wettability, minimizing pore and h-BN self reunion of h-BN and matrix, improve its mechanical property while keeping the excellent lubrication property of cutter material, reduce h-BN adds the adverse effect to self-lubrication ceramic cutter material mechanical property.In addition to being applicable to make self-lubrication ceramic cutter, it is also possible to be used for making ceramic die, bearing and other abrasion-proof corrosion-proof parts.
Accompanying drawing explanation
Fig. 1 is uncoated flake micron h-BN granule surface topography under scanning electron microscope.
Fig. 2 is the h-BN@SiO of preparation in embodiment 12Cladded type composite granule surface topography under scanning electron microscope.In figure, white particles is mono-dispersed nano SiO2Bead, for ease of observing, by the h-BN@SiO after cladding2Powder body grinds destruction part clad in agate mortar, it may be clearly seen that the fine and close clad covered on it is the clad of spherical nano-silicon dioxide composition.
Fig. 3 contrast experiment's example 1 directly adds the stereoscan photograph of the self-lubrication ceramic cutter material of h-BN, and in figure, tablet is h-BN, it can be seen that h-BN is combined not tight with matrix, occurs in that big pore, causes material compactness to decline.
Fig. 4 is that embodiment 1 adds h-BN@SiO2The stereoscan photograph of self-lubrication ceramic cutter material, in figure, h-BN is tightly combined with matrix, pore does not occur.
Detailed description of the invention
Below in conjunction with embodiment, technical solution of the present invention is further described.But the invention is not restricted to this.The Al used in embodiment2O3The mean diameter of powder is about 1 μm, and the mean diameter of TiC powder is about 0.5 μm, and MgO mean diameter is about 1 μm, and purity is all higher than 99%, is commercial products；The h-BN particle diameter used in embodiment is about 10 μm, and stereoscan photograph is as shown in Figure 1.Mill ball in embodiment is sintered carbide ball YG8.
Embodiment 1, the self-lubrication ceramic cutter material of interpolation spherical nano-silicon dioxide cladding hexagonal boron nitride composite granule, each component material percent by volume is: Al2O366.15%, TiC 28.35%, h-BN@SiO25%, MgO 0.5%.Preparation process is as follows:
(1)h-BN@SiO2The preparation of composite granule:
Weigh the h-BN micro-powder that 1g Average Particle Diameters is 10 μm to be scattered in 100mL dehydrated alcohol, ultrasonic disperse 10min, add 4.5mL distilled water and 4mL ammonia, pH value is about 8.5, proceeding in there-necked flask by the mixed liquor obtained, magnetic agitation heating in water bath, being heated to temperature is 45 DEG C.Keeping temperature 45 C, drip tetraethyl orthosilicate in above-mentioned mixed liquor, dropping mode is: 12mL tetraethyl orthosilicate is divided into 3 parts, a tetraethyl orthosilicate of dropping in 1.5h；With same titration mode second part of tetraethyl orthosilicate of dropping after 0.5h；Complete to start third time dropping after second time drips 0.5h；The like, tetraethyl orthosilicate amounts to point 3 times (4mL/ a time) and is slowly added dropwise in mixed liquor, and total reaction time is 6h.Reaction terminate after to the suspension obtained centrifugation 10min under the conditions of 2000r/min, with washes of absolute alcohol 3 times, under the conditions of 40 DEG C, obtain ball shaped nano SiO2Cladding flake micron h-BN composite granule h-BN SiO2。
Gained h-BN@SiO2Cladded type composite granule surface topography under scanning electron microscope is as shown in Figure 2.
(2) Al is taken in proportion2O3And TiC, and it is scattered in respectively in dehydrated alcohol, ultrasonic disperse mechanical agitation 25min, after being mixed by gained suspension, adds after MgO ultrasonic disperse mechanical agitation 25min, the complex phase suspension being uniformly mixed again；
(3) above-mentioned complex phase suspension is poured into ball milling fill, add sintered carbide ball, it is ensured that ball material weight ratio is 10:1, is filled with nitrogen as protective atmosphere continuous ball milling 48h；
(4) h-BN@SiO it is proportionally added into2By gained ball milling liquid continuous drying 36h at 110 DEG C in vacuum drying oven after composite granule ball milling 2h again, then sieve and obtain mixed powder, seal standby；
(5) step (4) gained dried mixed powder loading graphite jig will carry out hot pressed sintering, sintering temperature 1650 DEG C, hot pressing pressure 30MPa, temperature retention time 20min, 20 DEG C/min of programming rate.
Carrying out the prepared self-lubrication ceramic cutter material adding spherical nano-silicon dioxide cladding hexagonal boron nitride composite granule cutting into slices, coarse-fine mill, grind, polish, recording its mechanical property is: hardness 15.43GPa, fracture toughness 6.67MPa m1/2, bending strength 696MPa, coefficient of friction be 0.42.
Embodiment 2
Adding the self-lubrication ceramic cutter material of spherical nano-silicon dioxide cladding hexagonal boron nitride composite granule, each volume components percentage ratio is: Al2O362.65%, TiC 26.85%, h-BN@SiO210%, MgO 0.5%.Preparation process is as follows:
(1) with embodiment 1；
(2) appropriate Al is weighed in proportion2O3And TiC, and it is scattered in respectively in dehydrated alcohol, ultrasonic disperse mechanical agitation 20min, ultrasonic disperse mechanical agitation 20min, the complex phase suspension being uniformly mixed again after addition MgO after gained suspension is mixed；
(3) above-mentioned complex phase suspension is poured into ball milling fill, add sintered carbide ball, it is ensured that ball material weight ratio is 12:1, is filled with nitrogen as protective atmosphere continuous ball milling 48h；
(4) h-BN@SiO it is proportionally added into2By gained ball milling liquid continuous drying 24h at 120 DEG C in vacuum drying oven after composite granule ball milling 2.5h again, then sieve and obtain mixed powder, seal standby；
(5) the mixed powder loading graphite jig being dried by step (4) gained carries out hot pressed sintering, sintering temperature 1650 DEG C, hot pressing pressure 30MPa, temperature retention time 20min, 20 DEG C/min of programming rate.
Carrying out the prepared self-lubrication ceramic cutter material adding spherical nano-silicon dioxide cladding hexagonal boron nitride composite granule cutting into slices, coarse-fine mill, grind, polish, recording its mechanical property is: hardness 12.36GPa, fracture toughness 5.25MPa m1/2, bending strength 657MPa, coefficient of friction be 0.31.
Embodiment 3
Adding the self-lubrication ceramic cutter material of spherical nano-silicon dioxide cladding hexagonal boron nitride composite granule, each volume components percentage ratio is: Al2O347%, TiC 47%, h-BN@SiO25%, MgO 1%.Preparation process is as follows:
(1) with embodiment 1；
(2) Al is weighed in proportion2O3And TiC, and it is scattered in respectively in dehydrated alcohol, ultrasonic disperse mechanical agitation 15min, after being mixed by gained suspension, adds after appropriate MgO ultrasonic disperse mechanical agitation 15min, the complex phase suspension being uniformly mixed again；
(3) above-mentioned complex phase suspension is poured into ball milling fill, add sintered carbide ball, it is ensured that ball material weight ratio is 10:1, is filled with nitrogen as protective atmosphere continuous ball milling 36h；
(4) h-BN@SiO it is proportionally added into2By gained ball milling liquid continuous drying 48h at 100 DEG C in vacuum drying oven after composite granule ball milling 1.5h again, then sieve and obtain mixed powder, seal standby；
(5) step (4) gained dried mixed powder loading graphite jig will carry out hot pressed sintering, sintering temperature 1700 DEG C, hot pressing pressure 35MPa, temperature retention time 15min, 15 DEG C/min of programming rate.
Carrying out the prepared self-lubrication ceramic cutter material adding spherical nano-silicon dioxide cladding hexagonal boron nitride composite granule cutting into slices, coarse-fine mill, grind, polish, recording its mechanical property is: hardness 14.76GPa, fracture toughness 6.35MPa m1/2, bending strength 709MPa, coefficient of friction be 0.39.
Embodiment 4
Adding the self-lubrication ceramic cutter material of spherical nano-silicon dioxide cladding hexagonal boron nitride composite granule, each volume components percentage ratio is: Al2O350%, TiC 39.5%, h-BN@SiO210%, MgO 0.5%.Preparation method is as follows:
(1) with embodiment 1；
(2) with embodiment 1；
(3) above-mentioned complex phase suspension is poured into ball milling fill, add sintered carbide ball, it is ensured that ball material weight ratio is 8:1, is filled with nitrogen as protective atmosphere continuous ball milling 72h；
(4) h-BN@SiO it is proportionally added into2By gained ball milling liquid continuous drying 24h at 120 DEG C in vacuum drying oven after composite granule ball milling 3h again, then sieve and obtain mixed powder, seal standby；
(5) step (4) gained dried mixed powder loading graphite jig will carry out hot pressed sintering, sintering temperature 1600 DEG C, hot pressing pressure 25MPa, temperature retention time 30min, 10 DEG C/min of programming rate.
Carrying out the prepared self-lubrication ceramic cutter material adding spherical nano-silicon dioxide cladding hexagonal boron nitride composite granule cutting into slices, coarse-fine mill, grind, polish, recording its mechanical property is: hardness 12.35GPa, fracture toughness 5.43MPa m1/2, bending strength 672MPa, coefficient of friction be 0.29.
Contrast experiment's example
Contrast experiment's example 1:
Adding the self-lubrication ceramic cutter material of hexagonal boron nitride powder, each volume components percentage ratio is: Al2O366.15%, TiC 28.35%, h-BN 5%, MgO 0.5%.Preparation method is as follows:
(1) appropriate Al is weighed in proportion2O3And TiC, and it is scattered in respectively in dehydrated alcohol, ultrasonic disperse mechanical agitation 25min, after being mixed by gained suspension, adds after appropriate MgO ultrasonic disperse mechanical agitation 25min, the complex phase suspension being uniformly mixed again；
(2) above-mentioned complex phase suspension is poured into ball milling fill, add sintered carbide ball, it is ensured that ball material weight ratio is 10:1, is filled with nitrogen as protective atmosphere continuous ball milling 48h；
(3) it is proportionally added into gained ball milling liquid continuous drying 36h at 110 DEG C in vacuum drying oven after h-BN composite granule ball milling 2h again, then sieves and obtain mixed powder, seal standby；
(4) step (3) gained dried mixed powder loading graphite jig will carry out hot pressed sintering, sintering temperature 1650 DEG C, hot pressing pressure 30MPa, temperature retention time 20min, 20 DEG C/min of programming rate.
Carrying out the self-lubrication ceramic cutter material of prepared interpolation hexagonal boron nitride powder cutting into slices, coarse-fine mill, grind, polish, recording its mechanical property is: hardness 15.12GPa, fracture toughness 4.86MPa m1/2, bending strength 638MPa, coefficient of friction be 0.42.
Contrast experiment's example 2:
Adding the self-lubrication ceramic cutter material of hexagonal boron nitride powder, each volume components percentage ratio is: Al2O362.65%, TiC 26.85%, h-BN 10%, MgO 0.5%.Preparation method is as follows:
(1) appropriate Al is weighed in proportion2O3And TiC, and it is scattered in respectively in dehydrated alcohol, ultrasonic disperse mechanical agitation 20min, after being mixed by gained suspension, adds after appropriate MgO ultrasonic disperse mechanical agitation 20min, the complex phase suspension being uniformly mixed again；
(2) above-mentioned complex phase suspension is poured into ball milling fill, add sintered carbide ball, it is ensured that ball material weight ratio is 12:1, is filled with nitrogen as protective atmosphere continuous ball milling 48h；
(3) it is proportionally added into gained ball milling liquid continuous drying 24h at 120 DEG C in vacuum drying oven after h-BN composite granule ball milling 2.5h again, then sieves and obtain mixed powder, seal standby；
(4) step (3) gained dried mixed powder loading graphite jig will carry out hot pressed sintering, sintering temperature 1650 DEG C, hot pressing pressure 30MPa, temperature retention time 20min, 20 DEG C/min of programming rate.
Carrying out the self-lubrication ceramic cutter material of prepared interpolation hexagonal boron nitride powder cutting into slices, coarse-fine mill, grind, polish, recording its mechanical property is: hardness 12.11GPa, fracture toughness 4.32MPa m1/2, bending strength 605MPa, coefficient of friction be 0.30.
Respectively contrast experiment's example 1, contrast experiment's example 2 are compared discovery with embodiment 1, embodiment 2, under identical preparation process condition, add h-BN@SiO2The fracture toughness of self-lubrication ceramic cutter material and bending strength be significantly improved than the self-lubrication ceramic cutter material directly adding h-BN, and the hardness of material and coefficient of friction do not have significant change, therefore, the self-lubrication ceramic cutter material adding spherical nano-silicon dioxide cladding hexagonal boron nitride composite granule can significantly improve fracture toughness and the bending strength of material while keeping material lubrication property.
Claims (6)
1. the preparation method of the self-lubrication ceramic cutter material adding spherical nano-silicon dioxide cladding lamellar hexagonal boron nitride composite granule, it is characterised in that in described self-lubrication ceramic cutter material, each raw material components percent by volume is:
TiC 15-75%, h-BN@SiO22-20%, MgO 0.2-2.5%, remaining is Al2O3；
Comprise the following steps that
(1) h-BN@SiO2The preparation of composite granule:
In the dehydrated alcohol that the h-BN powder body that particle diameter is 1-20 μm is scattered in, h-BN is 0.5-10g:100-500mL with the mass volume ratio of dehydrated alcohol, ultrasonic disperse 10-30min, then add suitable quantity of water and to regulate pH value with the ammonia of mass fraction 23-28wt% be 8-9.5, by the mixed liquor magnetic agitation obtained heating in water bath, temperature is maintained at 30-70 DEG C；Being slowly added dropwise tetraethyl orthosilicate, h-BN is 0.5-10g:6-50mL with the mass volume ratio of tetraethyl orthosilicate, and tetraethyl orthosilicate rate of addition is 0.02-0.6 mL/min, and the response time is 2-24h；The suspension centrifugation 5-40min under the conditions of 1000-4000r/min that will obtain, with washes of absolute alcohol 2-5 time, is vacuum dried under the conditions of 40-100 DEG C, obtains with micron h-BN as core, Nano-meter SiO_22Preparing spherical SiO 2 for shell is coated with lamellar hexagonal boron nitride h-BN SiO2Composite granule；
(2) Al is taken in proportion2O3And TiC powder, it is scattered in respectively in dehydrated alcohol, ultrasonic disperse mechanical agitation 10-30min, by gained Al2O3Suspension adds MgO powder, again ultrasonic disperse mechanical agitation 10-30min, the complex phase suspension being uniformly mixed after mixing with TiC suspension；
(3) above-mentioned complex phase suspension being poured into ball milling fill, add sintered carbide ball, ball material mass ratio is 8-12:1, is filled with nitrogen or argon as protective atmosphere continuous ball milling 36-72h；
(4) h-BN@SiO it is proportionally added into2Composite granule ball milling 1-3h again, gained ball milling liquid continuous drying 24-48h at 100-120 DEG C in vacuum drying oven, then sieve and obtain mixed powder, seal standby；
(5) the mixed powder loading graphite jig being dried by step (4) gained carries out hot pressed sintering, sintering temperature 1600-1700 DEG C, hot pressing pressure 25-35MPa, temperature retention time 10-30min, programming rate 10-20 DEG C/min, to obtain final product.
2. the preparation method of self-lubrication ceramic cutter material as claimed in claim 1, it is characterised in that raw material components percent by volume is: the volumn concentration of described TiC is 25-50%；Described h-BN@SiO2Volumn concentration be 4-12%；The volumn concentration of described MgO is 0.4-1.2%.
3. the preparation method of self-lubrication ceramic cutter material as claimed in claim 1, it is characterised in that described Al2O3, TiC and MgO be micron order.
4. the preparation method of self-lubrication ceramic cutter material as claimed in claim 1, it is characterised in that described Al2O3The particle diameter of powder is 0.2-2 μm, and the particle diameter of TiC powder is 0.2-1.5 μm.
5. the preparation method of self-lubrication ceramic cutter material as claimed in claim 1, it is characterised in that described in step (1), water is distilled water, and amount of water is 0.5-10g:4-30mL with the mass volume ratio of h-BN.
6. the preparation method of self-lubrication ceramic cutter material as claimed in claim 1, it is characterised in that in step (2), h-BN is 1-5g:12mL-36mL with the mass volume ratio of tetraethyl orthosilicate；12mL-36mL tetraethyl orthosilicate is divided into 3 parts, in 1.5h, is slowly added dropwise the tetraethyl orthosilicate of a deal by several times；Continue reaction 0.5h for the first time after dropping, then second time drips the tetraethyl orthosilicate of a deal in the same way；After completing to drip for the second time, continuing reaction 0.5h, third time drips the tetraethyl orthosilicate of a deal the most in the same way；Third time continues reaction 0.5h after being added dropwise to complete, total reaction time is 6h.
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| CN106623908B (en) * | 2017-02-27 | 2018-11-13 | 齐鲁工业大学 | A kind of preparation method of nickel coated hexagonal boron nitride composite granule |
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| CN102815929B (en) * | 2012-09-10 | 2014-02-26 | 山东轻工业学院 | Multivariate gradient self-lubricating ceramic cutting tool material with surface having residual compressive stress and preparation method of multivariate gradient self-lubricating ceramic cutting tool material |
| CN103011784B (en) * | 2012-12-16 | 2014-08-06 | 山东轻工业学院 | High performance nano-composite aluminum oxide based self-lubricating cutter material and preparation method thereof |
| CN103058667B (en) * | 2013-01-17 | 2014-05-14 | 山东轻工业学院 | Nano solid lubricant and nano ceramic grain composite modified cutter material and preparation method thereof |
| CN104072146B (en) * | 2014-07-22 | 2015-10-14 | 江阴市赛英电子有限公司 | A kind of compound coating boron nitride-base polynary nanometer composite ceramics tool die material and preparation method thereof |
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| US10106412B2 (en) * | 2014-08-11 | 2018-10-23 | Hohai University | Method for preparing high-density hexagonal boron nitride ceramic material |
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